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Polyimide foam materiel and preparation method thereof

A technology of polyimide and foam materials, which is applied in the field of polyimide foam materials and its preparation, can solve problems such as foam collapse, foaming and foaming, and complicated preparation processes, and achieve simple and convenient production processes with low precursor Solution viscosity and the effect of reducing the amount of solvent

Active Publication Date: 2015-12-16
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In all the above-mentioned patents, the common point is that high-purity raw materials are required when synthesizing the precursor solution, so as to ensure that the raw materials fed are in an equimolar ratio, and the reaction temperature is strictly controlled to obtain a high-molecular-weight polyamic acid or polyester amine salt precursor. Bulk solution, otherwise, problems such as foaming, bubble collapse, shrinkage, etc. will easily occur during foaming due to the inability to obtain a precursor solution with a sufficiently high bulk viscosity, and the preparation process is complicated
However, in actual industrial operations, harsh reaction conditions, high raw material costs, and high-viscosity precursor solutions limit the popularization of polyimide foam materials. In addition, the process of crushing dry polyimide precursors for foaming, If the uniformity of the powder particle size cannot be well controlled, it will not be possible to prepare a foam with uniform cells

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1, prepare polyimide foam material

[0030] Prepare the polyimide foam material according to the following steps:

[0031] (1) Dissolve 31.02g (0.1mol) of 3,3',4,4'-diphenyl ether tetra-acid dianhydride in 25.6g of methanol, and react at reflux temperature (67°C) until clarification (2 hours), The reaction was continued for 1 hour to obtain a diacid diester solution.

[0032](2) Reduce the diacid diester solution obtained in step (1) to 40°C, add 20.24g (0.1mol) of 4'4-diaminodiphenyl ether, 102.4g tetrahydrofuran, 0.25g isoquinoline catalyst, and heat up to 60° C., reacted for 6 hours, added 1.03 g of polydimethylsiloxane, and continued to stir for 1 hour to obtain a polyimide precursor solution.

[0033] (3) Pour the precursor solution obtained in step (2) into a foaming mold and spread it flat, and dry it at room temperature (25°C). Pump down to 0.04MPa for 10 minutes, then pump down to 0.1MPa), keep for 24 hours and fully dry, then place the obtained p...

Embodiment 2

[0035] Embodiment 2, prepare polyimide foam material

[0036] Prepare the polyimide foam material according to the following steps:

[0037] (1) Dissolve 31.02g (0.1mol) of 3,3',4,4'-diphenyl ether tetra-acid dianhydride in 25.6g of methanol, and react at reflux temperature (67°C) until clarification (2 hours), The reaction was continued for 1 hour to obtain a diacid diester solution.

[0038] (2) Reduce the diacid diester solution obtained in step (1) to 40°C, add 20.24g (0.1mol), 3'4-diaminodiphenyl ether, 102.4g tetrahydrofuran, 0.5g pyridine catalyst, and heat up to 60 °C, reacted for 6 hours, added 1.03 g of polydimethylsiloxane, and continued to stir for 1 hour to obtain a polyimide precursor solution.

[0039] (3) Pour the precursor solution obtained in step (2) into a foaming mold and spread it flat, and dry it at room temperature (25°C). Pump down to 0.04MPa for 10 minutes, then pump down to 0.1MPa), keep for 24 hours and fully dry, then place the obtained polyimid...

Embodiment 3

[0041] Embodiment 3, prepare polyimide foam material

[0042] Prepare the polyimide foam material according to the following steps:

[0043] (1) Dissolve 31.02g (0.1mol) of 3,3',4,4'-diphenyl ether tetra-acid dianhydride in 25.6g of methanol, and react at reflux temperature (67°C) until clarification (2 hours), The reaction was continued for 1 hour to obtain a diacid diester solution.

[0044] (2) The diacid diester solution that step (1) obtains is down to 40 ℃, adds 20.24g (0.1mol) 4'4-diaminodiphenyl ether, 102.4g tetrahydrofuran, 0.25g isoquinoline catalyst, heats up to 60° C., reacted for 6 hours, added 1.03 g of polydimethylsiloxane, and continued to stir for 1 hour to obtain a polyimide precursor solution.

[0045] (3) Pour the precursor solution obtained in step (2) into a foaming mold and spread it flat, and dry it at room temperature (25°C). Pump down to 0.04MPa for 10 minutes, then pump down to 0.1MPa), keep for 24 hours and fully dry, then place the obtained pol...

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Abstract

The invention discloses a polyimide foam materiel and a preparation method thereof. The preparation method comprises the following steps: (1) mixing aromatic dianhydride with low molecular alcohol for an esterification reaction, so as to obtain a diacid diester solution; (2) mixing the diacid diester solution obtained in step (1) with a catalyst and furanidine for a reaction, so as to obtain a polyimide precursor solution; (3) drying the polyimide precursor solution obtained in step (2), carrying out foaming under vacuum and heating conditions to obtain a foaming intermediate, and conducting thermal imidization on the foaming intermediate to obtain the polyimide foam materiel. The polyimide foam materiel has the advantages that through adjustment of the temperature and the vacuum degree, the problem that in the prior art, the molecular mass of synthesized prepolymer powder is very low and causes foam combination in the conventional foaming process under the condition of very low material viscosity at foaming temperature can be effectively solved; meanwhile, the advantage that the precursor solution viscosity corresponding to the oligomer molecular mass is low can be kept, so that the polyimide foam materiel is easy to produce and process.

Description

technical field [0001] The invention relates to a polyimide foam material and a preparation method thereof, belonging to the field of polymer materials. Background technique [0002] Polyimide foam material is one of the research hotspots in recent years. The foam material has the characteristics of extreme temperature resistance (-250-450°C), radiation resistance, high flame retardancy, non-toxicity, oxidation resistance, hydrolysis resistance and the like. At the same time, the foamed polyimide material has low thermal conductivity and good sound absorption performance, and can be widely used in military and aerospace industries such as heat insulation for rockets, aircraft, aircraft carriers, submarines, etc., and civil flame retardant and heat insulation Fields such as insulation of high-temperature pipelines, etc. [0003] The research on polyimide foam material began in the 1960s. At that time, the Dupont company of the United States applied for the related patent US...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/10C08J9/02C08L79/08
Inventor 郭宝华丁光敏徐军
Owner TSINGHUA UNIV